反应详情

N1-Cyclobutanecarbonyl-N1-[4-(4-nitrophenoxy)-2-pyridyl]-1-cyclobutanecarboxamide (720 mg), iron powder (1.4 g), ammonium chloride (2.4 g), dimethylformamide (52 ml), ethanol (2 ml) and water (2 ml) were stirred at 100° C. for 15 minutes. The mixture was filtered with celite, and then water and ethyl acetate were added for extraction. The organic layer was washed 5 times with aqueous ammonium chloride solution and then dried over magnesium sulfate. The drying agent was filtered off, the solvent was distilled off under reduced pressure, ethyl acetate and hexane were added to the residue and the precipitated solid was filtered out to obtain 130 mg of a solid.

1. filtrationThe mixture was filtered with celite
2. additionwater and ethyl acetate were added for extraction
3. washThe organic layer was washed 5 times with aqueous ammonium chloride solution
4. dry with materialdried over magnesium sulfate
5. filtrationThe drying agent was filtered off
6. distillationthe solvent was distilled off under reduced pressure, ethyl acetate and hexane
7. additionwere added to the residue
8. filtrationthe precipitated solid was filtered out